CN103664163A - Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof - Google Patents
Medium for highly-dielectric grain boundary layer ceramic capacitor and preparation method thereof Download PDFInfo
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- CN103664163A CN103664163A CN201310463142.7A CN201310463142A CN103664163A CN 103664163 A CN103664163 A CN 103664163A CN 201310463142 A CN201310463142 A CN 201310463142A CN 103664163 A CN103664163 A CN 103664163A
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Abstract
The invention relates to the technical field of inorganic non-metallic materials, in particular to a medium for a highly-dielectric grain boundary layer ceramic capacitor and a preparation method thereof. The medium consists of the following components in percentage by weight: 88 to 96% of Ba(Ti0.9Sn0.1)O3, 0.1 to 3% of Ba(Yb1/2Nb1/2)O3, 0.1 to 4% of Dy2O3, 0.1 to 2.0% of SiO2, 0.1-2.5% of Al2O3, 0.03 to 4.0% of BaCO3, 0.1 to 2.0% of SiO2-Li2O-B2O3 glass frit (SLB) and 0.01 to 3% of CuO. The lead-free and cadmium-free medium for the highly-dielectric grain boundary layer ceramic capacitor is prepared from conventional chemical materials for the ceramic capacitor by adopting a conventional method for preparing a ceramic capacitor dielectric materials and a primary sintering process in the air and the sintering temperature of the ceramic capacitor is also reduced. The medium is suitable for preparing single-chip ceramic capacitors and monolithic ceramic capacitors.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, refer in particular to a kind of high mesomorphic interlayer ceramic capacitor dielectric and preparation method thereof, it adopts once sintered processing method in conventional ceramic capacitor dielectric preparation method and air, utilize condenser ceramics general chemistry raw material, prepare unleaded, the mesomorphic interlayer ceramic capacitor dielectric of height without cadmium, can also reduce the sintering temperature of condenser ceramics, this medium is suitable for preparing monolithic ceramic capacitor and individual layer chip ceramic capacitor, can greatly reduce the cost of ceramic condenser, this medium specific inductivity is high, easily realize the miniaturization of ceramic condenser, and good temp characteristic, proof voltage is high to expand the range of application of boundary ceramics electrical condenser simultaneously, and free from environmental pollution in preparation and use procedure, safe.
Background technology
Along with developing rapidly with universal of surface mounting technique, the occupation rate of surface mount component (SMC) in electronics steadily improves; 1997, World Developed Countries electronic devices and components chip rate reached more than 70%, and the whole world is average more than 40%; 2000, whole world electronic devices and components chip rate reached 70%; 2002, chip rate surpassed 85%; In particular for adapting to the national defence leading-edge fields such as message area and aerospace to small-size multifunction electronics device urgent need day by day, portability, miniaturization and the multifunction trend of complying with command, control, communications, and information terminal, electronic element has entered the all-round developing new period; Individual layer chip semiconductor ceramic material is divided into surperficial stratotype and crystal boundary stratotype two classes, is characterized in that volume is little, capacity is large.In addition, intergranular semiconductor stupalith also has that good temp characteristic, frequency response characteristic are good, operating frequency advantages of higher, at present in the world, only have AVX, JOHANSON etc. can provide individual layer chip semiconductor ceramic material less than ten companies, the whole world to the market aggregate demand of individual layer chip semiconductor ceramic material element up to 4,500,000,000/year, for adapting to an urgent demand day by day of electronic devices and components microminiaturization, lightness, Composite, high frequency and high performance, semiconductor ceramic material is in miniaturization, high-k, high precision int and high frequency aspect are developed rapidly, and individual layer chip semiconductor ceramic material is the trend of development, the sintering temperature of general monolithic boundary ceramics condenser dielectric and individual layer chip boundary ceramics condenser dielectric is 1350 ~ 1430 ℃, there are the following problems simultaneously: otherwise withstand voltage lower, temperature factor is larger, specific inductivity is lower, sintering process is all to adopt double sintering method substantially, that is: first high temperature reduction, then applies insulation oxide and carry out oxidizing thermal treatment in middle temperature, technique is more complicated, and cost is higher, some adopts cladding process, and technique is more complicated, and raw material is more expensive, and cost is also higher, and the mesomorphic interlayer ceramic capacitor dielectric of height of the present invention sintering temperature is 1280-1300 ℃ of left and right, adopt once sintered technique simultaneously, i.e. first binder removal before 500 ℃ in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30-50 ℃/h), then in 3-5 hour sintering of 1280-1300 ℃ of insulation, then be cooled to 900-950 ℃ of left and right in air, to be incubated processing in 2-3 hour, last furnace cooling, can greatly reduce the cost of boundary ceramics electrical condenser like this, the not leaded and cadmium of this patent capacitor ceramic dielectric simultaneously, condenser ceramics is free from environmental pollution in preparation and use procedure, in addition, the specific inductivity of condenser ceramics of the present invention is high, can improve like this capacity and the miniaturization of ceramic condenser, meets the development trend of ceramic condenser, equally also can reduce the cost of ceramic condenser, the mesomorphic interlayer ceramic capacitor dielectric of height of the present invention proof voltage is high, holds use range and security that requirement etc. that temperature characteristics meets X7R is conducive to expand boundary ceramics electrical condenser, is conducive to the miniaturization of ceramic condenser simultaneously.
Summary of the invention
The object of this invention is to provide a kind of high mesomorphic interlayer ceramic capacitor dielectric.
The object of the present invention is achieved like this:
High mesomorphic interlayer ceramic capacitor dielectric formula forms and comprises (weight percent): Ba (Ti
0.9sn
0.1) O
388-96%, Ba (Yb
1/2nb
1/2) O
30.1-3%, Dy
2o
30.1-4%, SiO
20.1-2.0%, Al
2o
30.1-2.5%, BaCO
30.03-4.0%, SiO
2-Li
2o-B
2o
3glass powder (SLB) 0.1-2.0%, CuO0.01-3%; Ba (Ti wherein
0.9sn
0.1) O
3, Ba (Yb
1/2nb
1/2) O
3, SiO
2-Li
2o-B
2o
3glass powder (SLB) is respectively to adopt conventional chemical feedstocks synthetic with solid phase method.
Ba (Ti used in medium of the present invention
0.9sn
0.1) O
3adopt following technique to prepare: by conventional chemical feedstocks BaCO
3and TiO
2and SnO
2press 1:0.9:0.1 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 1250 ℃, then cooling, obtains Ba (Ti after cooling
0.9sn
0.1) O
3, ground 200 mesh sieves, standby.
SiO used in medium of the present invention
2-Li
2o-B
2o
3glass powder (SLB) adopts following technique to prepare: by conventional chemical feedstocks SiO
2and Li
2cO
3and B
2o
3press 1:0.5:0.5 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 600-650 ℃, and quenching in water then obtains SiO after cooling
2-Li
2o-B
2o
3glass powder, ground 200 mesh sieves, standby.
Ba (Yb used in medium of the present invention
1/2nb
1/2) O
3adopt following technique to prepare: by conventional chemical feedstocks BaCO
3and Yb
2o
5and Nb
2o
5press 1:1/4:1/4 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 1250 ℃ of insulations 120 minutes, solid state reaction is synthesized Ba (Yb
1/2nb
1/2) O
3, ground 200 mesh sieves after cooling, standby.
The present invention adopts the mesomorphic interlayer ceramic capacitor dielectric of following high preparation technology: adopt conventional chemical feedstocks to synthesize respectively Ba (Ti with solid phase method
0.9sn
0.1) O
3, Ba (Yb
1/2nb
1/2) O
3, SiO
2-Li
2o-B
2o
3glass powder (SLB), then by formula batching, admixtion ball mill pulverizing is mixed, after drying, add tackiness agent granulation, be pressed into again green sheet, then in air, carry out binder removal and sintering, i.e. first binder removal 500 ℃ before in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30-50 ℃/h), then in 1280-1300 ℃, be incubated 3-5 hour sintering, then be cooled to 900-950 ℃ in air, to be incubated processing in 2-3 hour, last furnace cooling, obtain high mesomorphic interlayer ceramic capacitor dielectric, on medium by electrode.
Described dielectric withstanding voltage is higher, and direct current proof voltage is 6.2-6.9kV/mm; Specific inductivity is high, is 91183-92545; Dielectric loss is 106-139 * 10
-4; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic; Insulation resistance is 75-91 * 10
10Ω cm.
The formula of above-mentioned ceramic dielectic preferably adopts following two kinds of schemes (weight percent):
Ba (Ti
0.9sn
0.1) O
389-94%, Ba (Yb
1/2nb
1/2) O
30.3-2.5%, Dy
2o
30.3-2.5%, SiO
20.1-1.5%, Al
2o
30.1-2%, BaCO
30.05-1.6%, SiO
2-Li
2o-B
2o
3glass powder (SLB) 0.2-1.8%, CuO0.06-2%;
Ba (Ti
0.9sn
0.1) O
390-94%, Ba (Yb
1/2nb
1/2) O
30.3-2.0%, Dy
2o
30.3-2.0%, SiO
20.1-1.3%, Al
2o
30.1-1.6%, BaCO
30.08-1.5%, SiO
2-Li
2o-B
2o
3glass powder (SLB) 0.3-1.5%, CuO0.1-1.8%.
Compared with prior art, tool has the following advantages in the present invention:
1, the medium of this patent adopts following once sintered technique: first binder removal before 500 ℃ in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30-50 ℃/h), then in 3-5 hour sintering of 1280-1300 ℃ of insulation, then be cooled to 900-950 ℃ in air, to be incubated processing in 2-3 hour, last furnace cooling, can greatly reduce the cost of ceramic condenser like this, not leaded and cadmium in the media components of this patent, environmentally safe.
2, the specific inductivity of this medium is high, is more than 90000; Proof voltage is high, more than direct current proof voltage can reach 6kV/mm; Dielectric loss is little, is less than 1.5%; The specific inductivity of this medium is high, can realize miniaturization and the large capacity of ceramic condenser, can reduce costs equally.
3, the temperature factor of this medium is low, and percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic, and dielectric loss is less than 1.5%, and use procedure performance good stability is safe.
4, main raw material adopts the pure raw material of ceramic condenser level can produce ceramic dielectic of the present invention.
5, this medium adopts conventional solid phase method ceramic capacitor dielectric preparation technology and a reduction-oxidation sintering process to be prepared.
Embodiment
The invention will be further described in conjunction with the embodiments now.Table 1 provides the embodiments of the invention formula of totally 4 samples.
The embodiments of the invention main raw material of the formula of totally 4 samples adopt the pure raw material of ceramic condenser level, first adopt in the preparation conventional chemical feedstocks to synthesize respectively Ba (Ti with solid phase method
0.9sn
0.1) O
3, Ba (Yb
1/2nb
1/2) O
3, SiO
2-Li
2o-B
2o
3glass powder (SLB), then by above-mentioned formula batching, with distilled water or deionized water, adopt planetary ball mill ball milling to mix in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0) (mass ratio), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the polyvinyl alcohol solution that the concentration of its weight 8 ~ 10% is 10%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, first binder removal before 500 ℃ in nitrogen, then after higher than 1000 ℃ with heat up at a slow speed (30-50 ℃/h), then in 3-5 hour sintering of 1280-1300 ℃ of insulation, then be cooled to 900-950 ℃ in air, to be incubated processing in 2-3 hour, last furnace cooling, at 780 ~ 800 ℃, be incubated 15 minutes again and carry out silver ink firing, form silver electrode, solder taul again, seal, obtain high mesomorphic interlayer ceramic condenser, test its dielectric properties.
Above-mentioned dielectric properties of respectively filling a prescription sample are listed in table 2, and prepared condenser ceramics proof voltage is higher as can be seen from Table 2, more than direct current proof voltage can reach 6kV/mm; Specific inductivity is high, is more than 90000; Dielectric loss is less than 1.5 %; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic.
Table 1 embodiments of the invention are the formula of totally 4 samples
Respectively the fill a prescription dielectric properties of sample of table 2
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. a high mesomorphic interlayer ceramic capacitor dielectric, is characterized in that described medium composition according to weight percent calculating is: Ba (Ti
0.9sn
0.1) O
388-96%, Ba (Yb
1/2nb
1/2) O
30.1-3%, Dy
2o
30.1-4%, SiO
20.1-2.0%, Al
2o
30.1-2.5%, BaCO
30.03-4.0%, SiO
2-Li
2o-B
2o
3glass powder 0.1-2.0%, CuO0.01-3%; Ba (Ti wherein
0.9sn
0.1) O
3, Ba (Yb
1/2nb
1/2) O
3and SiO
2-Li
2o-B
2o
3glass powder adopts respectively conventional chemical feedstocks synthetic with solid phase method.
2. a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, is characterized in that: described dielectric withstanding voltage is higher, and direct current proof voltage is 6.2-6.9kV/mm; Specific inductivity is high, is 91183-92545; Dielectric loss is 106-139 * 10
-4; Percentage of capacitance variation with temperature is little, meets the requirement of X7R characteristic; Insulation resistance is 75-91 * 10
10Ω cm.
3. a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, is characterized in that: described Ba (Ti
0.9sn
0.1) O
3adopt following technique to prepare: by conventional chemical feedstocks BaCO
3and TiO
2and SnO
2press 1:0.9:0.1 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 1250 ℃, then cooling, obtains Ba (Ti after cooling
0.9sn
0.1) O
3, ground 200 mesh sieves, standby.
4. a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, is characterized in that: described SiO
2-Li
2o-B
2o
3glass powder adopts following technique to prepare: by conventional chemical feedstocks SiO
2and Li
2cO
3and B
2o
3press 1:0.5:0.5 molar ratio ingredient, ground and mixed is put into alumina crucible after evenly and is incubated 120 minutes in 600-650 ℃, and quenching in water then obtains SiO after cooling
2-Li
2o-B
2o
3glass powder, ground 200 mesh sieves, standby.
5. a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, is characterized in that: described Ba (Yb
1/2nb
1/2) O
3adopt following technique to prepare: by conventional chemical feedstocks BaCO
3and Yb
2o
5and Nb
2o
5press 1:1/4:1/4 molar ratio ingredient, after ground and mixed is even, put into alumina crucible in 1250 ℃ of insulations 120 minutes, solid state reaction is synthesized Ba (Yb
1/2nb
1/2) O
3, ground 200 mesh sieves after cooling, standby.
6. a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, described medium composition calculates according to weight percent and is: Ba (Ti
0.9sn
0.1) O
389-94%, Ba (Yb
1/2nb
1/2) O
30.3-2.5%, Dy
2o
30.3-2.5%, SiO
20.1-1.5%, Al
2o
30.1-2%, BaCO
30.05-1.6%, SiO
2-Li
2o-B
2o
3glass powder 0.2-1.8%, CuO0.06-2%.
7. a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, described medium composition calculates according to weight percent and is: Ba (Ti
0.9sn
0.1) O
390-94%, Ba (Yb
1/2nb
1/2) O
30.3-2.0%, Dy
2o
30.3-2.0%, SiO
20.1-1.3%, Al
2o
30.1-1.6%, BaCO
30.08-1.5%, SiO
2-Li
2o-B
2o
3glass powder 0.3-1.5%, CuO0.1-1.8%.
8. the preparation method of a kind of high mesomorphic interlayer ceramic capacitor dielectric as claimed in claim 1, is characterized in that comprising the steps: first to adopt conventional chemical feedstocks to synthesize respectively Ba (Ti with solid phase method
0.9sn
0.1) O
3, Ba (Yb
1/2nb
1/2) O
3, SiO
2-Li
2o-B
2o
3glass powder, then by formula batching, with distilled water or deionized water, adopt planetary ball mill ball milling to mix in the material preparing, material: ball: water=1:3:(0.6 ~ 1.0) (mass ratio), after ball milling 4 ~ 8 hours, dry to obtain dry mash, in dry mash, add and account for the polyvinyl alcohol solution that the concentration of its weight 8 ~ 10% is 10wt%, carry out granulation, mixed rear mistake 40 mesh sieves, under 20 ~ 30Mpa pressure, carry out again dry-pressing and become green sheet, first binder removal before 500 ℃ in nitrogen, then the speed with 30-50 ℃/h heats up after higher than 1000 ℃, then in 3-5 hour sintering of 1280-1300 ℃ of insulation, then be cooled to 900-950 ℃ in air, to be incubated processing in 2-3 hour, last furnace cooling, at 780 ~ 800 ℃, be incubated 15 minutes again and carry out silver ink firing, form silver electrode, solder taul again, seal, obtain high mesomorphic interlayer ceramic condenser.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (6)
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| CN105084892A (en) * | 2015-08-11 | 2015-11-25 | 电子科技大学 | High-medium single-layer miniature ceramic capacitor substrate material and preparation method thereof |
| CN105924150A (en) * | 2016-04-14 | 2016-09-07 | 江苏大学 | Low-temperature sintered conductive ceramic material and preparation method thereof |
| CN105967678A (en) * | 2016-04-29 | 2016-09-28 | 江苏大学 | Giant-dielectric ceramic capacitor medium and preparation method thereof |
| CN106518053A (en) * | 2015-09-10 | 2017-03-22 | 韩国机械研究院 | Crystal orientation template for BaTiO3-based lead-free piezoelectric ceramics and method for fabricating the same |
| CN106587989A (en) * | 2016-11-15 | 2017-04-26 | 江苏大学 | High-dielectric performance grain boundary layer ceramic capacitor medium |
| CN107117959A (en) * | 2017-06-23 | 2017-09-01 | 汕头市瑞升电子有限公司 | A kind of high-curie temperature PTC thermal sensitive ceramic materials and preparation method thereof |
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| CN105084892A (en) * | 2015-08-11 | 2015-11-25 | 电子科技大学 | High-medium single-layer miniature ceramic capacitor substrate material and preparation method thereof |
| CN105084892B (en) * | 2015-08-11 | 2017-09-01 | 电子科技大学 | High miniature ceramic capacitor substrate material of Jie's individual layer and preparation method thereof |
| CN106518053A (en) * | 2015-09-10 | 2017-03-22 | 韩国机械研究院 | Crystal orientation template for BaTiO3-based lead-free piezoelectric ceramics and method for fabricating the same |
| CN105924150A (en) * | 2016-04-14 | 2016-09-07 | 江苏大学 | Low-temperature sintered conductive ceramic material and preparation method thereof |
| CN105924150B (en) * | 2016-04-14 | 2018-08-21 | 江苏大学 | A kind of low sintering conducting ceramic material and preparation method thereof |
| CN105967678A (en) * | 2016-04-29 | 2016-09-28 | 江苏大学 | Giant-dielectric ceramic capacitor medium and preparation method thereof |
| CN105967678B (en) * | 2016-04-29 | 2019-04-02 | 江苏大学 | A kind of giant dielectric ceramic capacitor medium and preparation method thereof |
| CN106587989A (en) * | 2016-11-15 | 2017-04-26 | 江苏大学 | High-dielectric performance grain boundary layer ceramic capacitor medium |
| CN106587989B (en) * | 2016-11-15 | 2019-08-02 | 江苏大学 | A kind of high dielectric property grain boundary layer ceramic capacitor medium |
| CN107117959A (en) * | 2017-06-23 | 2017-09-01 | 汕头市瑞升电子有限公司 | A kind of high-curie temperature PTC thermal sensitive ceramic materials and preparation method thereof |
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